JP7356642B2 - Nickel hydroxide purification method - Google Patents
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Description
本発明は、リチウムイオン電池の正極材の原料として使用される水酸化ニッケルからマグネシウムを除去する技術に関する。 The present invention relates to a technique for removing magnesium from nickel hydroxide used as a raw material for positive electrode materials of lithium ion batteries.
二次電池であるリチウムイオン電池の正極材として、多種の正極材が開発されている。特に、近年では、従来使用されていたリチウム酸コバルトに代えて、三元系と呼ばれるニッケル・コバルト・マンガン（ＮＣＭ）系正極材や、ニッケル系と呼ばれるニッケル・コバルト・アルミニウム（ＮＣＡ）系等の正極材に注目が集まっている。 Various types of positive electrode materials have been developed as positive electrode materials for lithium ion batteries, which are secondary batteries. In particular, in recent years, instead of the conventionally used cobalt lithium oxide, cathode materials based on nickel-cobalt-manganese (NCM), which is called a ternary system, and nickel-cobalt-aluminum (NCA), which is called a nickel system, have been used. Cathode materials are attracting attention.
上述のようなニッケルやコバルトを含有する正極材は、例えば、ニッケル等の金属の塩を含有する溶液をアルカリで処理し、得られた金属水酸化物に焼成処理を施すことによって製造される。
このような金属塩としては、例えば、ニッケル酸化鉱石等を原料とするニッケル製錬工程で製造され、具体的には、塩化ニッケルや塩化コバルトなどの塩化物、硫酸ニッケルや硫酸コバルトなどの硫酸塩（硫酸ニッケル）等がある。
The positive electrode material containing nickel or cobalt as described above is manufactured, for example, by treating a solution containing a salt of a metal such as nickel with an alkali, and then subjecting the obtained metal hydroxide to a firing treatment.
Examples of such metal salts include chlorides such as nickel chloride and cobalt chloride, and sulfates such as nickel sulfate and cobalt sulfate. (nickel sulfate), etc.
なお、このうち、塩化物を用いた場合は、塩化物を中和し得られた水酸化物を焼成して酸化物とする際に、残留した塩化物イオンが塩素ガスとなり、焼成炉を腐食損傷することがあるなど環境や設備面での課題も多く、一般的には、金属塩には硫酸塩を用いることが多い。 In addition, when chloride is used, when the hydroxide obtained by neutralizing the chloride is fired to form an oxide, the remaining chloride ions become chlorine gas and corrode the firing furnace. There are many problems with the environment and equipment, such as the possibility of damage, and sulfates are generally used as the metal salt.
しかしながら、上述するニッケル酸化鉱石などの原料にはマグネシウムも含まれている場合が多い。また、ニッケル酸化鉱石からニッケルを酸浸出して抽出した場合、酸浸出で発生した過剰の酸を中和する段階や、得た硫酸ニッケルを中和したりして水酸化ニッケルを製造する段階で、酸化マグネシウムなどの中和剤を用いることが多く、その結果得た水酸化ニッケルなどの水酸化物にもマグネシウムが含まれることも多かった。 However, raw materials such as the above-mentioned nickel oxide ore often also contain magnesium. In addition, when nickel is extracted from nickel oxide ore by acid leaching, there is a step to neutralize the excess acid generated by acid leaching, and a step to produce nickel hydroxide by neutralizing the obtained nickel sulfate. , neutralizing agents such as magnesium oxide were often used, and the resulting hydroxides, such as nickel hydroxide, often contained magnesium.
しかしながらマグネシウムを含んだ水酸化ニッケルを原料に用いて焼成して酸化ニッケルを製造し、これを材料にＮＣＭ系正極材やＮＣＡ系正極材の正極材を製造すると、マグネシウムがそのまま残留して電池の電極中にマグネシウムが不純物として含まれることになる。
またマグネシウムにはリチウムイオン電池の充放電容量等の電池特性を低下させる性質があり、水酸化ニッケルに含有されることは好ましくなかった。
However, when nickel hydroxide containing magnesium is used as a raw material and fired to produce nickel oxide, and this material is used to produce cathode materials such as NCM-based cathode materials and NCA-based cathode materials, the magnesium remains as it is and the battery is damaged. Magnesium will be contained as an impurity in the electrode.
Furthermore, magnesium has the property of reducing battery characteristics such as charge/discharge capacity of lithium ion batteries, and it was not desirable for it to be contained in nickel hydroxide.
そのため、リチウムイオン電池の性能を維持向上させるためにも、マグネシウムの少ない高純度な水酸化ニッケルが求められてきた。
硫酸ニッケルや硫酸コバルト混合水溶液から不純物であるマグネシウムを分離するための公知の方法としては、硫化法、酸化中和法、溶媒抽出法等の方法が知られている。
Therefore, in order to maintain and improve the performance of lithium ion batteries, there has been a demand for highly pure nickel hydroxide that is low in magnesium.
Known methods for separating impurity magnesium from a mixed aqueous solution of nickel sulfate and cobalt sulfate include a sulfidation method, an oxidative neutralization method, and a solvent extraction method.
上記の方法の中で、硫化法及び酸化中和法については、ニッケルやコバルトを硫化物や水酸化物の形態で沈澱させ、濾過することにより、水溶液中に残留するマグネシウムと分離する技術である。
しかしながら、目的の溶液中に存在するニッケル及びコバルトの物量に対してマグネシウムの物量は一般には微量であるため、この微量のマグネシウムを除去するために、溶液中に大多数存在するニッケル及びコバルトを沈澱させることは、過大な硫化剤や中和剤及び酸化剤を使用することになり、経済的に有利とはいえない。
Among the above methods, the sulfurization method and the oxidative neutralization method are technologies in which nickel and cobalt are precipitated in the form of sulfides and hydroxides, and then filtered to separate them from the magnesium remaining in the aqueous solution. .
However, since the amount of magnesium is generally very small compared to the amount of nickel and cobalt present in the target solution, in order to remove this small amount of magnesium, the nickel and cobalt present in the majority of the solution are precipitated. Doing so requires the use of excessive amounts of sulfurizing agent, neutralizing agent, and oxidizing agent, which is not economically advantageous.
一方、溶媒抽出法は、各金属イオンを有機溶媒に抽出して抽残液に残留する他の金属イオンと分離する方法であり、抽出剤と抽出条件とを適切に設定することによって、不純物を選択的に除去することが可能となる利点がある。 On the other hand, the solvent extraction method is a method in which each metal ion is extracted into an organic solvent and separated from other metal ions remaining in the raffinate. Impurities are removed by appropriately setting the extractant and extraction conditions. It has the advantage of being able to be selectively removed.
例えば、特許文献１にあるような溶媒抽出法の従来技術を用いた場合、ニッケル及びコバルトを含んだ水溶液からマグネシウムを分離できる。具体的には特許文献１の図５におけるｐＨと抽出率の関係より、ｐＨを２．５～５．５の範囲に調整することで、有機溶媒中にコバルトやニッケルを抽出し、抽出されないマグネシウムと分離できる。
しかしながら、溶媒抽出を用いた場合でも、目的の溶液中に存在するニッケル及びコバルトの物量に対してマグネシウムの物量が圧倒的に微量となる場合は、微量のマグネシウムを除去するために、ニッケル及びコバルトを抽出させると、ニッケル及びコバルトの物量に相当するアルカリや酸などの薬剤が多大に要することになり、硫化法及び酸化中和法と同様にコストがかかる課題が依然として解消されなかった。
For example, when using the conventional technique of solvent extraction as disclosed in
However, even when solvent extraction is used, if the amount of magnesium is overwhelmingly small compared to the amount of nickel and cobalt present in the target solution, nickel and cobalt may be added to remove the trace amount of magnesium. Extracting nickel and cobalt requires a large amount of chemicals such as alkalis and acids corresponding to the amount of nickel and cobalt, and the problem of high costs, similar to the sulfurization method and the oxidation neutralization method, has not been resolved.
一方で、非特許文献１にあるような、ビス（２－エチルヘキシル）ホスファートを抽出剤として使用すれば、ニッケルやコバルトよりも優先的にマグネシウムが抽出されることが知られており、このビス（２－エチルヘキシル）ホスファートを使用することで、リチウムイオン電池の正極材に使用可能となる品位にまでマグネシウムを分離することができる。
On the other hand, it is known that when bis(2-ethylhexyl) phosphate is used as an extractant, as described in Non-Patent
けれども、リチウムイオン電池の需要が急拡大を続け、これに伴う競争の激化に対応して、高品質な水酸化ニッケルをより低コストに得る方法が引き続き求められてきた。 However, in response to the rapidly expanding demand for lithium-ion batteries and the resulting intensification of competition, there continues to be a need for a method to obtain high-quality nickel hydroxide at a lower cost.
本発明は、マグネシウムを含むニッケル水酸化物からより低コストにマグネシウムを分離しようとするものである。 The present invention aims to separate magnesium from nickel hydroxide containing magnesium at a lower cost.
上記の課題を解決するための本発明の第１の発明は、ニッケルとマグネシウムを含む水酸化物を、洗浄液と混合、撹拌して、該洗浄液との混合スラリーのｐＨを７．５～８．５の範囲で維持するように、該洗浄液のｐＨを制御しつつ、混合スラリーを形成しながら洗浄を行った後、得られた前記混合スラリーを固液分離処理して洗浄後液と洗浄物を得る１次洗浄工程と、次いで、前記１次洗浄工程で得られた洗浄物に、硫酸溶液を添加して前記洗浄物を浸出する硫酸浸出工程で得られた浸出スラリーを、固液分離処理して浸出液と浸出残渣に分離後、分離した前記浸出液を溶媒抽出工程に付して硫酸ニッケル溶液を得、次いで前記硫酸ニッケル溶液にアルカリを添加する中和処理に付してマグネシウム含有量を低減した水酸化ニッケルを得ることを特徴とする水酸化ニッケルの精製方法である。 A first aspect of the present invention to solve the above-mentioned problems is to mix a hydroxide containing nickel and magnesium with a cleaning liquid, stir it , and adjust the pH of the mixed slurry with the cleaning liquid to 7.5 to 8. After washing while forming a mixed slurry while controlling the pH of the washing solution so as to maintain the pH within the range of A leaching slurry obtained in a sulfuric acid leaching step of adding a sulfuric acid solution to the washed material obtained in the first washing step and leaching the washed material is subjected to solid-liquid separation treatment. After separation into leachate and leach residue, the separated leachate was subjected to a solvent extraction process to obtain a nickel sulfate solution, and then subjected to a neutralization process by adding an alkali to the nickel sulfate solution to reduce the magnesium content. This is a method for purifying nickel hydroxide, which is characterized by obtaining nickel hydroxide.
本発明の第２の発明は、第１の発明における洗浄液が、電気伝導率２００μS／ｃｍ以下、且つｐＨが６．５～８．５の範囲の水であることを特徴とする水酸化ニッケルの精製方法である。 A second invention of the present invention is a cleaning liquid of nickel hydroxide according to the first invention, characterized in that the cleaning liquid is water having an electrical conductivity of 200 μS/cm or less and a pH in the range of 6.5 to 8.5. This is a purification method.
本発明の第３の発明は、第１の発明における洗浄液が、ｐＨが７．５～８．５の水溶液であることを特徴とする水酸化ニッケルの精製方法である。 A third invention of the present invention is a method for purifying nickel hydroxide, characterized in that the cleaning liquid according to the first invention is an aqueous solution having a pH of 7.5 to 8.5 .
本発明の第４の発明は、ニッケルとマグネシウムを含む水酸化物を、ｐＨ７．５～８．５の水溶液からなる洗浄液と混合、撹拌してｐＨ６．５を超える混合スラリーを形成しながら洗浄を行った後、得られた前記混合スラリーを固液分離処理して洗浄後液と洗浄物を得る１次洗浄工程と、次いで、前記１次洗浄工程で得られた洗浄物に、硫酸溶液を添加して前記洗浄物を浸出する硫酸浸出工程で得られた浸出スラリーを、固液分離処理して浸出液と浸出残渣に分離後、分離した前記浸出液を溶媒抽出工程に付して硫酸ニッケル溶液を得、次いで前記硫酸ニッケル溶液にアルカリを添加する中和処理に付してマグネシウム含有量を低減した水酸化ニッケルを得ることを特徴とする水酸化ニッケルの精製方法である。 The fourth aspect of the present invention is to perform cleaning while forming a mixed slurry having a pH of over 6.5 by mixing and stirring a hydroxide containing nickel and magnesium with a cleaning solution consisting of an aqueous solution having a pH of 7.5 to 8.5. After that, a primary cleaning step in which the obtained mixed slurry is subjected to solid-liquid separation treatment to obtain a washed liquid and a cleaning product, and then a sulfuric acid solution is added to the cleaning product obtained in the primary cleaning step. The leaching slurry obtained in the sulfuric acid leaching step in which the washed material is leached is subjected to solid-liquid separation treatment to be separated into a leachate and a leaching residue, and then the separated leachate is subjected to a solvent extraction step to obtain a nickel sulfate solution. This is a method for purifying nickel hydroxide, which is characterized in that the nickel hydroxide solution is then subjected to a neutralization treatment by adding an alkali to the nickel sulfate solution to obtain nickel hydroxide with a reduced magnesium content .
本発明によれば、マグネシウムを含有する水酸化ニッケルを溶媒抽出工程に付して精製する際に、工程にかかる負荷を低減させ、併せて溶媒抽出にかかる薬剤コストも低減可能となる。その結果リチウムイオン電池の正極材の原料として使用できる濃度までマグネシウム濃度を低減させた硫酸ニッケル溶液を効率よく精製できる。本発明を用いることで、従来よりも効率よく低コストに水酸化ニッケルに含有されるマグネシウムを分離できるようになった。 According to the present invention, when nickel hydroxide containing magnesium is purified by subjecting it to a solvent extraction process, the load on the process can be reduced, and the cost of chemicals required for the solvent extraction can also be reduced. As a result, it is possible to efficiently purify a nickel sulfate solution in which the magnesium concentration is reduced to a concentration that can be used as a raw material for the positive electrode material of lithium ion batteries. By using the present invention, it has become possible to separate magnesium contained in nickel hydroxide more efficiently and at lower cost than before.
本発明は、溶媒抽出技術を用いたプロセスをより安価に提供する為に、溶媒抽出に付す前にマグネシウムを除去、低減する工程適用可能な方法であり、出発原料を（予備洗浄としての）１次洗浄を行ってマグネシウムを除去し、低減しておく方法に関するもので、マグネシウムは出発原料の水酸化物中では水溶性物質を形成していると、大きなマグネシウムの低減効果が得られる。 The present invention is an applicable process for removing and reducing magnesium before subjecting it to solvent extraction, in order to provide a process using solvent extraction technology at a lower cost. This relates to a method of removing and reducing magnesium by performing subsequent washing, and if magnesium forms a water-soluble substance in the hydroxide of the starting material, a large magnesium reduction effect can be obtained.
具体的には、マグネシウムを含んだ固体の水酸化ニッケル（ニッケルおよびマグネシウムを含む水酸化物に相当）に洗浄液を添加して撹拌するなどしてスラリーとし、このスラリーのｐＨを適切な範囲に維持することで、水酸化ニッケル中のマグネシウムを洗浄液（洗浄後液）中に浸出しながら、同時に水酸化ニッケル中のニッケルが浸出されるロスを抑制するものである。 Specifically, a cleaning liquid is added to solid nickel hydroxide containing magnesium (equivalent to hydroxide containing nickel and magnesium) and stirred to form a slurry, and the pH of this slurry is maintained within an appropriate range. By doing so, while the magnesium in the nickel hydroxide is leached into the cleaning solution (washing solution), at the same time, the loss of nickel in the nickel hydroxide is suppressed.
通常、マグネシウムや、その他の不純物を含んだ粗原料ともいうべき水酸化ニッケル(以下「ＭＨＰ」と称する)は、一度硫酸で溶解して硫酸ニッケル溶液を得ることが行われるが、この溶解の際には、ＭＨＰ中のニッケルは硫酸ニッケルとして溶液中に浸出させ、一方不要成分であるマグネシウムは溶液中に浸出させないことが好ましい。 Normally, nickel hydroxide (hereinafter referred to as "MHP"), which can be called a crude raw material containing magnesium and other impurities, is once dissolved in sulfuric acid to obtain a nickel sulfate solution. For this purpose, it is preferable that nickel in MHP is leached into the solution as nickel sulfate, while magnesium, which is an unnecessary component, is not leached into the solution.
ここで、本発明者がＭＨＰを硫酸で浸出する際のｐＨとニッケルおよびマグネシウムの浸出率を検討したところ、図１に示すように、ニッケルは概ねｐＨが５以下での領域ではほぼ１００％浸出されるが、ｐＨが５を超えて上昇するに従って浸出率が急激に低下し、ｐＨ７．５では１％程度しか浸出されず、ｐＨ８．５ではほとんど浸出されなくなる。一方、マグネシウムはｐＨが６．５程度までは７０～８０％程度が浸出され、それ以上のｐＨでも概ね４０％程度の浸出率が得られている。 Here, when the present inventor investigated the pH and the leaching rate of nickel and magnesium when leaching MHP with sulfuric acid, as shown in Figure 1, nickel was leached out at almost 100% in the pH range of 5 or less. However, as the pH rises above 5, the leaching rate decreases rapidly; at pH 7.5, only about 1% is leached, and at pH 8.5, almost no leaching occurs. On the other hand, about 70 to 80% of magnesium is leached out up to a pH of about 6.5, and even at higher pHs, a leaching rate of about 40% is obtained.
このことから、１次洗浄において、洗浄に加える洗浄液とＭＨＰから形成されたスラリーのｐＨを７．５以上に維持するようにスラリーのｐＨ、又は添加する洗浄液のｐＨを管理しながら洗浄することで、マグネシウムの約４０％を洗浄後の洗浄液（洗浄後液）に分配させ、ＭＨＰから除去できることを見出した。
なお、この場合のニッケルの浸出率、つまりニッケルロスは０．５～１％となる。このニッケルロスが１％を超えても許容できる場合は、ｐＨが７前後の水を用いた洗浄でもよく、ニッケルロスを０．５％未満まで絞る場合は、ｐＨが８～８．５あるいはそれ以上のアルカリ性の洗浄液を用いることでマグネシウムを除去できる。
From this, in the primary cleaning, it is possible to clean by controlling the pH of the slurry or the pH of the cleaning liquid to be added so that the pH of the slurry formed from the cleaning liquid added to the cleaning and MHP is maintained at 7.5 or higher. It was discovered that about 40% of magnesium can be distributed to the post-washing solution (post-washing solution) and removed from the MHP.
In this case, the leaching rate of nickel, that is, the nickel loss, is 0.5 to 1%. If this nickel loss exceeds 1% but is acceptable, washing with water with a pH of around 7 may be sufficient.If the nickel loss is to be reduced to less than 0.5%, the pH should be 8 to 8.5 or higher. Magnesium can be removed by using the above alkaline cleaning solution.
このように、溶媒抽出工程に付す前に１次洗浄してマグネシウムを分離しておくことで、その後の溶媒抽出工程での段数や抽出剤の量を低減することが可能となり、工数や設備投資や使用する薬剤のコストを圧縮することが可能となる。 In this way, by first washing and separating magnesium before subjecting it to the solvent extraction process, it is possible to reduce the number of stages and amount of extractant in the subsequent solvent extraction process, reducing man-hours and equipment investment. It becomes possible to reduce the cost of medicines and drugs used.
以下、実施例を用い、本発明を説明する。
先ず、一次洗浄工程における混合スラリーのｐＨ範囲は、以下のようにして求めた。
ニッケルを４１．７重量％、マグネシウムを１．８重量％含む表１に示す成分組成の水酸化ニッケルを１サンプルに付き２０ｇ分取し、次いで分取した水酸化ニッケルを純水２００ｍｌと共にビーカーに入れて撹拌した。これを１サンプルとして、各サンプルに６４重量％の硫酸を添加してｐＨを１．０～８．５の間でそれぞれの数値に調整して維持した。１時間撹拌後、全量を濾過し、得た濾液の液量、残渣量、濾液に含まれるニッケル、マグネシウム量を測定し浸出率を求めた。
Hereinafter, the present invention will be explained using Examples.
First, the pH range of the mixed slurry in the primary cleaning step was determined as follows.
20g of nickel hydroxide having the composition shown in Table 1 containing 41.7% by weight of nickel and 1.8% by weight of magnesium was collected per sample, and then the collected nickel hydroxide was placed in a beaker with 200ml of pure water. and stirred. This was treated as one sample, and 64% by weight of sulfuric acid was added to each sample to adjust and maintain the pH at a respective value between 1.0 and 8.5. After stirring for 1 hour, the entire amount was filtered, and the amount of the obtained filtrate, the amount of residue, and the amount of nickel and magnesium contained in the filtrate were measured to determine the leaching rate.
その結果、ｐＨを７．５以上に維持して１次洗浄することで、ニッケルロスを１％未満に抑制しながらマグネシウムの４０％を分離することができ、その分、後工程である溶媒抽出工程でのマグネシウム負荷を低減できる。 As a result, by maintaining the pH at 7.5 or higher and performing the first wash, it is possible to separate 40% of magnesium while suppressing nickel loss to less than 1%, which is offset by the subsequent solvent extraction. The magnesium load in the process can be reduced.
上記試験結果を基に、水酸化ニッケルの精製を実施した。
先ず、上記水酸化ニッケルを１００ｇ分取し、その水酸化ニッケルと純水との混合スラリーを作製し、その混合スラリーを撹拌しながら、そのｐＨが７．５～８．５の間に維持されるように、ｐＨ調整剤として水酸化ナトリウムや６４重量％硫酸を適宜添加し、１時間撹拌する水酸化物の１次洗浄工程を実施した。
所定時間終了後、アスピレータと濾過鐘を用いた吸引濾過により、その全量を固液分離して洗浄後液と洗浄物を得た。
Based on the above test results, nickel hydroxide was purified.
First, 100 g of the above nickel hydroxide was collected, a mixed slurry of the nickel hydroxide and pure water was prepared, and the mixed slurry was stirred to maintain its pH between 7.5 and 8.5. Sodium hydroxide and 64% by weight sulfuric acid were appropriately added as pH adjusters, and a hydroxide primary washing step was carried out in which the mixture was stirred for 1 hour.
After a predetermined period of time, the entire amount was separated into solid and liquid by suction filtration using an aspirator and a filter bell to obtain a washed liquid and a washed product.
分離した洗浄物に６４重量％硫酸溶液を添加し、ニッケルを浸出する硫酸浸出工程、その後の固液分離処理を経て、浸出液と浸出残渣に分離後、分離した浸出液を、抽出剤にビス（２－エチルへキシル）ホスファート（Ｄ２ＥＨＰＡ）を用いた溶媒抽出工程に供して作製した硫酸ニッケル溶液に、水酸化ナトリウム水溶液（アルカリ）を添加する中和処理を施し、マグネシウム含有量を０．４５ｗｔ％未満に低減した水酸化ニッケル（沈殿物）を得た。 A 64% by weight sulfuric acid solution is added to the separated washed material, followed by a sulfuric acid leaching step in which nickel is leached out, followed by a solid-liquid separation treatment to separate the leachate and leach residue. A nickel sulfate solution prepared by subjecting it to a solvent extraction process using -ethylhexyl)phosphate (D2EHPA) is neutralized by adding an aqueous sodium hydroxide solution (alkali) to reduce the magnesium content to less than 0.45 wt%. nickel hydroxide (precipitate) was obtained.
（比較例１）
１次洗浄工程における撹拌されている混合スラリーのｐＨ範囲を、６．０以上、６．５未満に維持した以外は実施例１と同じ条件で水酸化ニッケルの精製を実施した。
その結果、マグネシウム含有量は実施例１と比較して低減されず、さらにニッケルロスも抑制されなかった。
(Comparative example 1)
Nickel hydroxide was purified under the same conditions as in Example 1, except that the pH range of the mixed slurry being stirred in the primary washing step was maintained at 6.0 or more and less than 6.5.
As a result, the magnesium content was not reduced compared to Example 1, and furthermore, nickel loss was not suppressed.
Claims (4)
次いで、前記１次洗浄工程で得られた洗浄物に、硫酸溶液を添加して前記洗浄物を浸出する硫酸浸出工程で得られた浸出スラリーを、固液分離処理して浸出液と浸出残渣に分離後、分離した前記浸出液を溶媒抽出工程に付して硫酸ニッケル溶液を得、次いで前記硫酸ニッケル溶液にアルカリを添加する中和処理に付してマグネシウム含有量を低減した水酸化ニッケルを得ることを特徴とする水酸化ニッケルの精製方法。 A hydroxide containing nickel and magnesium is mixed with a cleaning liquid and stirred, while controlling the pH of the cleaning liquid so that the pH of the mixed slurry with the cleaning liquid is maintained in the range of 7.5 to 8.5. , a primary cleaning step of performing washing while forming a mixed slurry, and then subjecting the obtained mixed slurry to solid-liquid separation treatment to obtain a washed liquid and a washed product;
Next, a sulfuric acid solution is added to the washed material obtained in the primary washing step to leach out the washed material.The leaching slurry obtained in the sulfuric acid leaching step is subjected to solid-liquid separation treatment to separate it into a leachate and a leached residue. After that, the separated leachate is subjected to a solvent extraction step to obtain a nickel sulfate solution, and then subjected to a neutralization treatment by adding an alkali to the nickel sulfate solution to obtain nickel hydroxide with a reduced magnesium content. Characteristic method for refining nickel hydroxide.
次いで、前記１次洗浄工程で得られた洗浄物に、硫酸溶液を添加して前記洗浄物を浸出する硫酸浸出工程で得られた浸出スラリーを、固液分離処理して浸出液と浸出残渣に分離後、分離した前記浸出液を溶媒抽出工程に付して硫酸ニッケル溶液を得、次いで前記硫酸ニッケル溶液にアルカリを添加する中和処理に付してマグネシウム含有量を低減した水酸化ニッケルを得ることを特徴とする水酸化ニッケルの精製方法。 A hydroxide containing nickel and magnesium is mixed with a cleaning solution consisting of an aqueous solution having a pH of 7.5 to 8.5, and the mixture is washed while stirring to form a mixed slurry with a pH of over 6.5. a primary cleaning step in which the slurry is subjected to solid-liquid separation treatment to obtain a washed liquid and a washed product;
Next, a sulfuric acid solution is added to the washed material obtained in the primary washing step to leach out the washed material.The leaching slurry obtained in the sulfuric acid leaching step is subjected to solid-liquid separation treatment to separate it into a leachate and a leached residue. After that, the separated leachate is subjected to a solvent extraction step to obtain a nickel sulfate solution, and then subjected to a neutralization treatment by adding an alkali to the nickel sulfate solution to obtain nickel hydroxide with a reduced magnesium content. Characteristic method for refining nickel hydroxide.
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